Reverse detergent



Patented Feb. 10, 1948 aiasnzs nnvmsa DETERGENT" Will rd 111.1 Kirkpatrick and D me" L Wilson, 4 Sug ar,-;Lant1, -,Teg. assignors tto Niscolroducts Gompapy, lipuston,{lex., atcorporationpfllelar Mario Drawing; ApplicationNovember-5222,1944; :semmo. 564,113

elevated=tempenaturea =in=mostiinst nces will still retain: w asadeflnite chemical eontam-ination with water-nor other hydrophili'c' body; the :presence of which can" be ascertained by =-the -factth'at it is not readily wetted with oil. Another instance'is the -oil dru-ms used to sh -p 'both lubricatingand fuel "oils; Especially w-h'en these are used for transoceanic sl-ripment; -afterthey have been emetiedstheyarc ik'ely-to-beseriously soiled or contaminated;bothinside and outside "It: is not 9 11 1192}. to h atthem with steam jets of very hot steam and to rinse themwith caustic. either with or without a reliminary steam heating. In th s way. it is possible toeliminate-practically all the contamination except the residual water contam nat on-left after theapplication of caustic or any other aqueous solution.-

In rx nstances such traces .of '.water are more orless objectionablesnmetimes to suchnn ex lentrast prevent further use of. the container the surface in a condition such that the hydro-' phobic material subsequently placed in contac with the container or machine part will readily wet it and find not even a chemical trace of water present at the contact surface.

In preparing one suitable reagent for the practice oi the invention we employ the following ingradients:

1. Amyl naphthalene: A mixture of monoamyland diamyl-naphthalenes having the following specifications:

Sp. G. at 20 0.94-0.96 M. W 231-56 angler distillation by AS'IM method D-86-35 i2, modinedas.outlinedinISharples;standardth'am. tic rin'st-ruet nns,

-1 cc. not below 250 6; 95% between 250-=4003 'C;

:2. .Isopropanol Regular 99 ,commer.cial-giiade..

:3.;-Sulurie 1 acid; Re ular I -98 commercial grade; I

A; Coumarone a indene fraction: A distillate fraction-20f coal: tarrcommonly known as' heavy solvent naphtha :boiling; between 160 -200" 0. l and having a minimum polymerizable.eontent'pi 30 as lzdeterminedtzbytmethod .of Ellis '& Rabinowitz,

described-in-flour; Indz'Eng'; Chem.,18, {797 (1916) .5. iicyclohexylaminez-w eltegular commercial. grade:

1.6; Ammonia:- Regular it 26% Bij commercial grade '7. Gas oil-z' (lommcnzcommercialigrade.

TO::D1'0d11C8 arreagent iaccordine- {to -the invention, 2625 :pounds 1Of1t amylnaplithalene and 13-27, pounds of.;isopropanol:are mixed and 480 pounds of 198%wsulfuricacid is ,dded :3 l3 a; temperature not exceeding 45 1-01 Su fonation ,is :carried put at a temperature of -150 to 55 (3. by maintaining atzthis -.tempenatureaf0r two hours to yield an alkylatede naphthalene sulfonic acid The free acid is then :washed out day dumping the reaction product into cold water while cooline to keep the temperature below 80 C. The amount "of cold water used. .is'isueh' that the l final wash water at room temperature should'not be less than 38 B. norl more than -.4lB. About i000 pounds of water-willrusuallytgive a;result within the limits stated, 1200=.-pounds .of a petroleum ,fraction' which .we designate .gas oil and which is not much different than a high boiling kerosene is usually added in the washing process. This permits a more ready stratific tion of the two layers. After settling vernight, the clear upper layer is recovered and amounts to about 5500 to 6000 pounds. A convenient way to do this is to drain off the wash water which constitutes the lower layer, leavina the upper layer in the process kettle. To this, 3'75 pounds of cyclohexylamine is added and the temperature is brought up to 0., whereby the basic amine reacts with the alkylated naphthalene sulfonic acid to reduce the acidity 110 to 150 gallons of water are addedand thor-' oughly stirred. The acid Wash water is allowed to settle and discharged to waste and the residual acidity of the mass is neutralized to methyl orange alkalinity with 26 B. ammonia. This usually requires approximately 475 pounds of the ammonia. The ammonium sulfate solution is allowed to settle out and if necessary the product is brightened by heating to about 105 C. to remove any water present in suspension. This completes the product and it is now ready for packaging and in a batch of the size given amounts to about 6800 pounds.

The proportions of the different ingredients may be varied considerably, Without attempting to state definitely just what the extreme limits are, it is stated that, beginning with 2625 lbs. of amylnaphthalene, the isopropanol may be from 275 to 330 pounds. The sulfuric acid is present in excess and therefore the amount can be indefinite. The petroleum fraction may be between 1000 and 1400 pounds; the cyclohexylamine may be from 360 to 460. pounds; and the coumarone indene fraction from 1000 to 1200 pounds. The 150 gallons of water is merely wash water and therefore the amount is indefinite.

The final product disclosed herein ha a specific gravity of 1.02. It is not injured by limited exposure to the atmosphere, but prolonged and extreme exposure will cause it to dry out much as varnish does. Small amounts of water will blend into the mass and do no harm, and large amounts will settle out after prolonged standing. It has a characteristic odor suggestive of coal tar products and is stable up to 130 C. It has a. viscosity or "body similar to a light lube oil,

The material is best prepared for actual use by dissolving it in suitable hydrocarbon solvent for ease in application and handling. Such solvents as benzene, toluene, unleaded gasoline, kerosene, naphtha, gas oil, fuel oil, Diesel oil, bunker oil, and various alcohols, ketones, chlorinated aliphatics, organic sulphides, and carbon tetrachloride may be employed.

The ratio or the reagent to solvent may vary from somewhat less than 1% to essentially 100% reagent, depending upon conditions. For instance, for the general rinsing of drums or containers, a 5% solution of the reagent in ordinary commercial unleaded gasoline functions very Well, but if the containers to be treated are heavily coated with water, a higher-percentageiis preferable so that therinse will not be exhausted too quickly.

After an extended period of use, the rinse will merely become weak and when this occurs it can be setaside and a layer containing substantially percent water together with only traces of reagent will accumulate at the bottom on standing and can be drained off. Similarly, where treatment is by dipping parts in a reservoir, the bottom of the vessel is best formed with a sump and a valve to drain the same and the accumulated water may be drained off from time to time without interrupting the use of the bath. Water thus drained off contains such small amount of the reagent that the loss is negligible, and treatment to recover the reagent is not worth while.

Without further elaboration the foregoing will so full explain our invention that others may readily adapt the same for use under various conditions of service.

We claim:

1. The method of'conditioning surfaces foruse under conditions such that traces of water constitute a contaminant, which comprises rinsing the surfaces with a non-aqueous rinse consisting of a non-aqueous hydrophobic organic'solvent in which is dissolved an oil soluble amine salt of a coumarone-indene resin modified alkylated naph- REFERENCES CITED The following references are of record in the file of this patent:

UNITED STATES PATENTS Number Name Date 2,262,926 Edgar et al, Nov. 18, 1941 2,137,404 Hollerer Nov, 24, 1938 2,130,668 Gunther Sept. 20, 1938 2,206,589 Wayne July 2, 1940 2,139,276 Lenher et a1. Dec. 6, 1938 2,055,588 Pospiech Sept. 29, 1936 

